Peeling Experiments Of Ductile Thin Films Along Ceramic Substrates - Critical Assessment Of Analytical Models

Two types of peeling experiments are performed in the present research. One is for the Al film/Al2O3 substrate system with an adhesive layer between the film and the substrate. The other one is for the Cu film/Al2O3 substrate system without adhesive layer between the film and the substrate, and the Cu films are electroplated onto the Al2O3 substrates. For the case with adhesive layer, two kinds of adhesives are selected, which are all the mixtures of epoxy and polyimide with mass ratios 1:1.5 and 1:1, respectively. The relationships between energy release rate, the film thickness and the adhesive layer thickness are measured during the steady-state peeling process. The effects of the adhesive layer on the energy release rate are analyzed. Using the experimental results, several analytical criteria for the steady-state peeling based on the bending model and on the two-dimensional finite element analysis model are critically assessed. Through assessment of analytical models, we find that the cohesive zone criterion based on the beam bend model is suitable for a weak interface strength case and it describes a macroscale fracture process zone case, while the two-dimensional finite element model is effective to both the strong interface and weak interface, and it describes a small-scale fracture process zone case. (C) 2007 Elsevier Ltd. All rights reserved.

Determination of interface properties between micron-thick metal film and ceramic substrate using peel test

Peel test measurements have been performed to estimate both the interface toughness and the separation strength between copper thin film and Al2O3 substrate with film thicknesses ranging between 1 and 15 mu m. An inverse analysis based on the artificial neural network method is adopted to determine the interface parameters. The interface parameters are characterized by the cohesive zone (CZ) model. The results of finite element simulations based on the strain gradient plasticity theory are used to train the artificial neural network. Using both the trained neural network and the experimental measurements for one test result, both the interface toughness and the separation strength are determined. Finally, the finite element predictions adopting the determined interface parameters are performed for the other film thickness cases, and are in agreement with the experimental results.

Small scale, grain size and substrate effects in nano-indentation experiment of film-substrate systems

The mechanical properties of film-substrate systems have been investigated through nano-indentation experiments in our former paper (Chen, S.H., Liu, L., Wang, T.C., 2005. Investigation of the mechanical properties of thin films by nano-indentation, considering the effects of thickness and different coating-substrate combinations. Surf. Coat. Technol., 191, 25-32), in which Al-Glass with three different film thicknesses are adopted and it is found that the relation between the hardness H and normalized indentation depth h/t, where t denotes the film thickness, exhibits three different regimes: (i) the hardness decreases obviously with increasing indentation depth; (ii) then, the hardness keeps an almost constant value in the range of 0.1-0.7 of the normalized indentation depth h/t; (iii) after that, the hardness increases with increasing indentation depth. In this paper, the indentation image is further investigated and finite element method is used to analyze the nano-indentation phenomena with both classical plasticity and strain gradient plasticity theories. Not only the case with an ideal sharp indenter tip but also that with a round one is considered in both theories. Finally, we find that the classical plasticity theory can not predict the experimental results, even considering the indenter tip curvature. However, the strain gradient plasticity theory can describe the experimental data very well not only at a shallow indentation depth but also at a deep depth. Strain gradient and substrate effects are proved to coexist in film-substrate nano-indentation experiments. (c) 2006 Elsevier Ltd. All rights reserved.

I. Anisotropy and crystal structure of ferromagnetic thin films. II. Investigations into magnetic microstructure by Lorentz microscopy

The induced magnetic uniaxial anisotropy of Ni-Fe alloy films has been shown to be related to the crystal structure of the film. By use of electron diffraction, the crystal structure or vacuum-deposited films was determined over the composition range 5% to 85% Ni, with substrate temperature during deposition at various temperatures in the range 25° to 500° C. The phase diagram determined in this way has boundaries which are in fair agreement with the equilibrium boundaries for bulk material above 400°C. The (α+ ɤ) mixture phase disappears below 100°C.

The measurement of uniaxial anisotropy field for 25% Ni-Fe alloy films deposited at temperatures in the range -80°C to 375°C has been carried out. Comparison of the crystal structure phase diagram with the present data and those published by Wilts indicates that the anisotropy is strongly sensitive to crystal structure. Others have proposed pair ordering as an important source of anisotropy because of an apparent peak in the anisotropy energy at about 50% Ni composition. The present work shows no such peak, and leads to the conclusion that pair ordering cannot be a dominant contributor.

Width of the 180° domain wall in 76% Ni-Fe alloy films as a function of film thickness up to 1800 Å was measured using the defocused mode of Lorentz microscopy. For the thinner films, the measured wall widths are in good agreement with earlier data obtained by Fuchs. For films thicker than 800 Å, the wall width increases with film thickness to about 9000 Å at 1800 Å film thickness. Similar measurements for polycrystalline Co films with thickness from 200 to 1500 Å have been made. The wall width increases from 3000 Å at 400 Å film thickness to about 6000 Å at 1500 Å film thickness. The wall widths for Ni-Fe and Co films are much greater than predicted by present theories. The validity of the classical determination of wall width is discussed, and the comparison of the present data with theoretical results is given.

Finally, an experimental study of ripple by Lorentz microscopy in Ni-Fe alloy films has been carried out. The following should be noted: (1) the only practical way to determine experimentally a meaningful wavelength is to find a well-defined ripple periodicity by visual inspection of a photomicrograph. (2) The average wavelength is of the order of 1µ. This value is in reasonable agreement with the main wavelength predicted by the theories developed by others. The dependence of wavelength on substrate deposition temperature, alloy composition and the external magnetic field has been also studied and the results are compared with theoretical predictions. (3) The experimental fact that the ripple structure could not be observed in completely epitaxial films gives confirmation that the ripple results from the randomness of crystallite orientation. Furthermore, the experimental observation that the ripple disappeared in the range 71 and 75% Ni supports the theory that the ripple amplitude is directly dependent on the crystalline anisotropy. An attempt to experimentally determine the order of magnitude of the ripple angle was carried out. The measured angle was about 0.02 rad. The discrepancy between the experimental data and the theoretical prediction is serious. The accurate experimental determination of ripple angle is an unsolved problem.

Optical parameters and absorption of copper (II)-azo complexes thin films as optical recording media

Smooth thin films of three kinds of azo dyes of 2-(5'-tert-butyl-3'-azoxylisoxazole)-1, 3-diketones and their copper (II)-azo complexes were prepared by the spin-coating method. Absorption spectra of the thin films on a glass substrate in the 300-600 nm wavelength region were measured. Optical constants (complex refractive index N=n+ik) and thickness of the thin films prepared on single-crystal silicon substrate in the 300-600 nm wavelength region were investigated on rotating analyzer-polarizer type of scanning ellipsometer, and dielectric constants epsilon(epsilon=epsilon(1)+i epsilon(2)), absorption coefficients alpha as well as reflectance R of thin films were then calculated. In addition, one of the copper (II)-azo complex thin film prepared on glass substrate with an Ag reflective layer was also studied by atomic force microscopy (AFM) and static optical recording. AFM study shows that the copper (II)-azo complex thin film is very smooth and has a root mean square surface roughness of 1.89 nm. Static optical recording shows that the recording marks on the copper (II)-azo complex thin film are very clear and circular, and the size of the minimal recording marks can reach 200 nm. (c) 2004 Elsevier B.V. All rights reserved.

Determination and analysis of the optical constants of thin films of nickel(II) and copper(II) hydrazone complexes by spectroscopic ellipsometry

Thin films of four nickel(II) and copper(II) hydrazone complexes, which will hopefully be used as recording layers for the next-generation of high-density recordable disks, were prepared by using the spin-coating method. Absorption spectra of the thin films on K9 optical glass substrates in the 300-700 nm wavelength region were measured. Optical constants (complex refractive indices N) and thickness d of the thin films prepared on single-crystal silicon substrates in the 275-675 nm wavelength region were investigated on a rotating analyzer-polarizer scanning ellipsometer by fitting the measured ellipsometric angles (Psi(lambda) and Delta(lambda)) with a 3-layer model (Si/dye film/air). The dielectric functions epsilon and absorption coefficients alpha as a function of the wavelength were then calculated. Additionally, a design to achieve high reflectivity and optimum dye film thickness with an appropriate reflective layer was performed with the Film Wizard software using a multilayered model (PC substrate/reflective layer/dye film/air) at 405 nm wavelength.

Optical properties of nickel(II)-azo complexes thin films for potential application as high-density recordable optical recording media

Smooth thin films of three kinds of nickel(II)-azo complexes were prepared by the spin-coating method. Absorption spectra of the thin films on K9 glass substrate in the 300-600 nn wavelength region were measured. Optical constants (complex refractive index N = n + ik) and thickness of the thin films prepared on single-crystal silicon substrate in the 300-600 nm wavelength region were investigated on rotating analyzer-polarizer type of scanning ellipsometer, and dielectric constants epsilon (epsilon = epsilon(1) + i epsilon(2)), absorption coefficients a as well as reflectance R of thin films were then calculated at 405 nm. In addition, in order to examine the possible use of nickel(II)-azo complex thin film as an optical recording medium, one of the nickel(II)-azo complex thin film prepared on K9 glass substrate with an Ag reflective layer was also studied by atomic force microscopy and static optical recording. The results show that the nickel(II)-azo complex thin film is smooth and has a root mean square surface roughness of 2.25 nm, and the recording marks on the nickel(II)-azo complex thin film are very clear and circular, and their size can reach 200 nn or less. (c) 2006 Elsevier Ltd. All rights reserved.

Thickness dependence of structure and optical properties of silver films deposited by magnetron sputtering

A series of silver films with different thickness were prepared under identical conditions by direct current magnetron sputtering. The optical properties of the silver films were measured using spectrophotometric techniques and the optical constants were calculated from reflection and transmission measurements made at near normal incidence. The results show that the optical properties and constants are affected by films' thickness. Below the critical thickness of 17 nm at which Ag film forms a continuous film, the optical properties and constants vary significantly as the thickness of films increases and then tends to a stable value which is reached at 41 nm. X-ray diffraction measurements were carried out to examine the structure and stress evolution of the Ag films as a function of films' thickness. It was found that the interplanar distance of (111) orientation decreases when the film thickness increases and tends to be close to that of bulk material. The compressive strains also decrease with increasing thickness. (C) 2007 Published by Elsevier B.V.

Optical properties and microstructure of Ta2O5 biaxial film

This study investigates the optical properties and microstructure of Ta2O5 film deposited with the glancing angle deposition technique. The tilted nanocolumn microstructure, examined with scanning electron microscopy, induces the optical anisotropy of thin film. The optical properties of thin film are characterized with an inverse synthesis method. Based on the Cauchy model, the dispersion equations of optical constants of film are determined from the transmittance spectra measured at normal and oblique incidence over 400-800 nm. The starting values derived with an envelope method quicken the optimization process greatly. The dispersion of the principal indices N-1, N-2, and N-3 and the thickness d of thin film are presented statistically. A good agreement between the measured optical properties and theoretical calculation is obtained, which validates the model established for thin film produced by glancing angle deposition. (C) 2008 Optical Society of America

Rolling of thin strip and foil: Application of a tribological model for "mixed" lubrication

A mechanical model of cold rolling of foil is coupled with a sophisticated tribological model. The tribological model treats the "mixed" lubrication regime of practical interest, in which there is "real" contact between the roll and strip as well as pressurized oil between the surfaces. The variation of oil film thickness and contact ratio in the bite is found by considering flattening of asperities on the foil and the build-up of hydrodynamic pressure through the bite. The boundary friction coefficient for the contact areas is taken from strip drawing tests under similar tribological conditions. Theoretical results confirm that roll load and forward slip decrease with increasing rolling speed due to the decrease in contact ratio and friction. The predictions of the model are verified using mill trials under industrial conditions. For both thin strip and foil, the load predicted by the model has reasonable agreement with the measurements. For rolling of foil, forward slip is overestimated. This is greatly improved if a variation of friction through the bite is considered.

Deposition and characterisation of ultralow-stress ZnO thin films for application in FBAR-based gravimetric biosensors

Zinc oxide (ZnO) thin films were deposited at high rates ( > 50 nm min-1) using a unique technique known as high target utilisation sputtering (HiTUS). The films obtained possess good crystallographic orientation, low surface roughness, very low stress and excellent piezoelectric properties. We have utilised the films to develop highly sensitive biosensors based on thickness longitudinal mode (TLM) thin film bulk acoustic resonators (FBARs). The FBARs have the fundamental TLM at a frequency near 1.5 GHz and quality factor Q higher than 1,000, which is one of the largest values ever reported for ZnO-based FBARs. Bovine Serum Albumin (BSA) solutions with different concentrations were placed on the top of different sets of identical FBARs and their responses to mass-loading from physically adsorbed protein coatings were investigated. These resonators demonstrated a high sensitivity and thus have a great potential as gravimetric sensors for biomedical applications. © 2011 Inderscience Enterprises Ltd.

In situ intercalation dynamics in inorganic-organic layered perovskite thin films.

The properties of layered inorganic semiconductors can be manipulated by the insertion of foreign molecular species via a process known as intercalation. In the present study, we investigate the phenomenon of organic moiety (R-NH3I) intercalation in layered metal-halide (PbI2)-based inorganic semiconductors, leading to the formation of inorganic-organic (IO) perovskites [(R-NH3)2PbI4]. During this intercalation strong resonant exciton optical transitions are created, enabling study of the dynamics of this process. Simultaneous in situ photoluminescence (PL) and transmission measurements are used to track the structural and exciton evolution. On the basis of the experimental observations, a model is proposed which explains the process of IO perovskite formation during intercalation of the organic moiety through the inorganic semiconductor layers. The interplay between precursor film thickness and organic solution concentration/solvent highlights the role of van der Waals interactions between the layers, as well as the need for maintaining stoichiometry during intercalation. Nucleation and growth occurring during intercalation matches a Johnson-Mehl-Avrami-Kolmogorov model, with results fitting both ideal and nonideal cases.

Fracture Properties of LPCVD Silicon Nitride and Thermally Grown Silicon Oxide Thin Films From the Load-Deflection of Long Si3N4 and SiO2/Si3N4 Diaphragms

The bulge test is successfully extended to the determination of the fracture properties of silicon nitride and oxide thin films. This is achieved by using long diaphragms made of silicon nitride single layers and oxide/nitride bilayers, and applying comprehensive mechanical model that describes the mechanical response of the diaphragms under uniform differential pressure. The model is valid for thin films with arbitrary z-dependent plane-strain modulus and prestress, where z denotes the coordinate perpendicular to the diaphragm. It takes into account the bending rigidity and stretching stiffness of the layered materials and the compliance of the supporting edges. This enables the accurate computation of the load-deflection response and stress distribution throughout the composite diaphragm as a function of the load, in particular at the critical pressure leading to the fracture of the diaphragms. The method is applied to diaphragms made of single layers of 300-nm-thick silicon nitride deposited by low-pressure chemical vapor deposition and composite diaphragms of silicon nitride grown on top of thermal silicon oxide films produced by wet thermal oxidation at 950 degrees C and 1050 degrees C with target thicknesses of 500, 750, and 1000 mn. All films characterized have an amorphous structure. Plane-strain moduli E-ps and prestress levels sigma(0) of 304.8 +/- 12.2 GPa and 1132.3 +/- 34.4 MPa, respectively, are extracted for Si3N4, whereas E-ps = 49.1 +/- 7.4 GPa and sigma(0) = -258.6 +/- 23.1 MPa are obtained for SiO2 films. The fracture data are analyzed using the standardized form of the Weibull distribution. The Si3N4 films present relatively high values of maximum stress at fracture and Weibull moduli, i.e., sigma(max) = 7.89 +/- 0.23 GPa and m = 50.0 +/- 3.6, respectively, when compared to the thermal oxides (sigma(max) = 0.89 +/- 0.07 GPa and m = 12.1 +/- 0.5 for 507-nm-thick 950 degrees C layers). A marginal decrease of sigma(max) with thickness is observed for SiO2, with no significant differences between the films grown at 950 degrees C and 1050 degrees C. Weibull moduli of oxide thin films are found to lie between 4.5 +/- 1.2 and 19.8 +/- 4.2, depending on the oxidation temperature and film thickness.

Thickness dependent dislocation, electrical and optical properties in InN films grown by MOCVD

InN thin films with different thicknesses are grown by metal organic chemical vapor deposition, and the dislocations, electrical and optical properties are investigated. Based on the model of mosaic crystal, by means of X-ray diffraction skew geometry scan, the edge dislocation densities of 4.2 x 10(10) cm(-2) and 6.3 x 10(10) cm(-2) are fitted, and the decrease of twist angle and dislocation density in thicker films are observed. The carrier concentrations of 9 x 10(18) cm(-3) and 1.2 x 10(18) cm(-3) are obtained by room temperature Hall effect measurement. V-N is shown to be the origin of background carriers, and the dependence of concentration and mobility on film thickness is explained. By the analysis of S-shape temperature dependence of photoluminescence peak, the defects induced carrier localization is suggested be involved in the photoluminescence. Taking both the localization and energy band shrinkage effect into account, the localization energies of 5.05 meV and 5.58 meV for samples of different thicknesses are calculated, and the decrease of the carrier localization effect in the thicker sample can be attributed to the reduction of defects.

Study on growth mechanism of low-temperature prepared microcrystalline Si thin films

Microcrystalline silicon thin films at different growth stages were prepared by hot wire chemical vapor deposition. Atomic force microscopy has been applied to investigate the evolution of surface topography of these films. According to the fractal analysis I it was found that, the growth of Si film deposited on glass substrate is the zero-diffused stochastic deposition; while for the film on Si substrate, it is the finite diffused deposition on the initial growth stage, and transforms to the zero-diffused stochastic deposition when the film thickness reaches a certain value. The film thickness dependence of island density shows that a maximum of island density appears at the critical film thickness for both substrates. The data of Raman spectra approve that, on the glass substrate, the a-Si: H/mu c-Si:H transition is related to the critical film thickness. Different substrate materials directly affect the surface diffusion ability of radicals, resulting in the difference of growth modes on the earlier growth stage.